Studies On The Synthesis Of The Plasticizer DEDB?EIMB And Pharmaceutical Intermediate MMMB

DEDB is a novel environmental plasticizer.Using p-toluene sulfonic acid as catalyst,ethylene glycol dibenzoate was prepared through the esterification of benzoic acid with ethylene glycol in the presence of cyclohexane as the water carrier.The effect of molar ratio of acid to glycol,amount of catalyst,cyclohexane dosage and reacon time on the yield were studied.The optimum reaction conditions were as follows:n(benzoic acid):n(diethylene glycol)=2.0:1.1,catalyst dosage 3.0%,cyclohexane 12 mL and reaction time 8 h,taking acetone-water(V/V=1:1)as hydrolysis system and hydrolysis time 3 h.The yield of the target product was 98.0%.Ethyl 3-isopropyl-2-(methoxymethyl)benzoate is a novel engineering plasticizer widely used in fields such as aircraft industry.The compound was prepared through six steps,with 3-bromo-2-methylbenzoic acid as a starting material.The key step of the synthetic route lies on the Suzuki-Coupling reaction in the fifth step.The novel compounds MMMB,an intermediate used to synthesize an inhibitor of the Varicella Zoster virus,was prepared from 2-methoxybenzoyl chloride through ten steps.Sitafloxacin(DU-6859a,STFX)is a novel antibacterial Quinolone,which has a very strong broad-spectrum antibacterial ability because of its more balanced dual inhibiting effect on the DNA spiral enzyme(spirase)and topoisomerase IV of bacteria.The synthetic route of an intermediate of Sitafloxacin,(S)-tert-butyl 5-azaspiro[2.4]heptan-7-ylcarbamate,was studied.Atorvastatin calcium is the global best-selling blood lipid regulator.For ensuring the medicinal safety and quality,it is necessary to determine the impurities and degradation products of pharmaceutical active substances.It is essential to provide standards of these compounds to perform the exact quantitative analysis.The impurity was prepared through the Paal-Knorr Furan Synthesis and photoxidation starting from 2-(2-(4-fluorophenyl)-2-oxo-1-phenylethyl)-4-methyl-3-oxo-N-phenylpentanamide that was used to prepare Atorvastatin calcium.